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A kind of preparation method of doxycycline hydrochloride impurity c

A technology of doxycycline hydrochloride and impurities, which is applied in the preparation of carboxylic acid amide optical isomers, organic chemistry and other directions, can solve the problems of low yield of impurity C, low efficiency, small sample size, etc., and achieve a large amount of impurity C. , the effect of high purity

Active Publication Date: 2018-12-14
绍兴市逸晨医疗科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The literature discloses a preparation of doxycycline hydrochloride impurity C (preparation of doxycycline hydrochloride impurity C and research on antibacterial activity and toxicity in vitro, Journal of China Pharmaceutical University, 2016), but the method has a low yield of impurity C ( about 10%), and what it uses is the preparative liquid phase, and the sample loading amount of the preparative liquid phase is small, needs repeated separation repeatedly, and efficiency is low

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  • A kind of preparation method of doxycycline hydrochloride impurity c

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Effect test

Embodiment 1

[0023] The preparation of embodiment 1 doxycycline hydrochloride impurity C

[0024] Including the following steps:

[0025] Step S1, high temperature treatment:

[0026] First take by weighing doxycycline hydrochloride raw material 100mg, add tetrahydrofuran aqueous solution and dissolve and make doxycycline hydrochloride solution, the volume percentage composition of tetrahydrofuran in the tetrahydrofuran aqueous solution is 25%, and the concentration of doxycycline hydrochloride solution is 10mg / mL, then Treat in a boiling water bath for 2.5 hours, concentrate and remove THF in the solution after cooling, and finally freeze-dry to obtain a high-temperature-treated sample;

[0027] Step S2, high-speed countercurrent chromatographic separation:

[0028] Prepare ethyl acetate-ethanol-water-glacial acetic acid (5:2:6:0.04, v / v / v / v) solvent system 12 hours before separation. The specific preparation method is: mix the four solvents in proportion and shake vigorously Finally, ...

Embodiment 2

[0031] The preparation of embodiment 2 doxycycline hydrochloride impurity C

[0032] Including the following steps:

[0033] Step S1, high temperature treatment:

[0034] First take by weighing doxycycline hydrochloride raw material 100mg, add tetrahydrofuran aqueous solution and dissolve and make doxycycline hydrochloride solution, the volume percentage composition of tetrahydrofuran in tetrahydrofuran aqueous solution is 15%, and the concentration of doxycycline hydrochloride solution is 8mg / mL, then Treat in a boiling water bath for 2 hours, concentrate and remove THF in the solution after cooling, and finally freeze-dry to obtain a high-temperature-treated sample;

[0035] Step S2, high-speed countercurrent chromatographic separation:

[0036] Prepare ethyl acetate-ethanol-water-glacial acetic acid (5:2:6:0.04, v / v / v / v) solvent system 12 hours before separation. The specific preparation method is: mix the four solvents in proportion and shake vigorously Finally, let it ...

Embodiment 3

[0039] The preparation of embodiment 3 doxycycline hydrochloride impurity C

[0040] Including the following steps:

[0041] Step S1, high temperature treatment:

[0042] First take doxycycline hydrochloride raw material 100mg, add tetrahydrofuran aqueous solution and dissolve and make doxycycline hydrochloride solution, the volume percentage composition of tetrahydrofuran in the tetrahydrofuran aqueous solution is 35%, and the concentration of doxycycline hydrochloride solution is 12mg / mL, then Treat in a boiling water bath for 3 hours, concentrate and remove THF in the solution after cooling, and finally freeze-dry to obtain a high-temperature-treated sample;

[0043] Step S2, high-speed countercurrent chromatographic separation:

[0044] Prepare ethyl acetate-ethanol-water-glacial acetic acid (5:2:6:0.04, v / v / v / v) solvent system 12 hours before separation. The specific preparation method is: mix the four solvents in proportion and shake vigorously Finally, let it stand f...

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Abstract

The invention discloses a preparation method of doxycycline hydrochloride impurity C. The preparation method comprises the following steps: step S1, high-temperature treatment: firstly weighing a doxycycline hydrochloride raw material, dissolving by a tetrahydrofuran aqueous solution to obtain a doxycydine hydrochloride solution, wherein a volume percent fraction of tetrahydrofuran in the tetrahydrofuran aqueous solution is 15 to 35 percent, treating for 2 to 3 h in a boiling water bath, cooling, concentrating, removing the tetrahydrofuran in the solution, and finally freeze drying to obtain a high-temperature processed sample; and step S2, high-speed countercurrent chromatographic separation: dissolving the high-temperature processed sample by utilizing a fixed phase and a flow phase of a same volume to be used as a sample solution, and adopting ethyl acetate-ethanol-water-glacial acetic acid (5 to 2 to 6 to 0.04, v / v / v / v) as a two-phase solvent system, wherein an upper phase is a fixed phase, a lower phase is a flow phase, and corresponding components of the impurity C are collected according to a chromatogram under the condition that the rotation speed of a host machine is 800 r / min, the flow rate is 2.0 mL / min, and the detection wavelength is 268 nm. The method provided by the invention is high in preparation efficiency, and the purity of the impurity C is improved.

Description

technical field [0001] The invention belongs to the field of medicine, and relates to a preparation method of an impurity reference substance, in particular to a preparation method of doxycycline hydrochloride impurity C. Background technique [0002] The literature discloses a preparation of doxycycline hydrochloride impurity C (preparation of doxycycline hydrochloride impurity C and research on antibacterial activity and toxicity in vitro, Journal of China Pharmaceutical University, 2016), but the method has a low yield of impurity C ( About 10%), and what it uses is the preparative liquid phase, and the sample loading amount of the preparative liquid phase is small, needs repeated separation repeatedly, and efficiency is low. Contents of the invention [0003] The object of the present invention is to provide a kind of preparation method of doxycycline hydrochloride impurity C, to improve the preparation efficiency of impurity C. [0004] The present invention is achie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/16C07C231/20C07C237/26
CPCC07C231/16C07C231/20C07C237/26
Inventor 陈云孟梓瑄王斌
Owner 绍兴市逸晨医疗科技有限公司